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Aluminum metal organic framework materials

a technology of organic frameworks and metals, applied in the direction of group 3/13 element organic compounds, group 4/14 element organic compounds, etc., can solve the problems of low chemical stability, hampering the application of the industry, and few stable mofs, especially in single crystal form, and achieve excellent solubility, excellent starting materials, and high symmetry

Active Publication Date: 2015-08-11
TEXAS A&M UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This approach enables the production of aluminium MOFs with crystal sizes exceeding previous limits, achieving high chemical and mechanical stability, and enhanced gas adsorption capabilities, overcoming the challenges of low crystallinity and small particle sizes in existing synthesis methods.

Problems solved by technology

However, one of the limitations of most MOFs is their low chemical stability, which undoubtedly hampers their application in industry.
This method has become the focus of some recent research efforts but very few stable MOFs have been obtained, especially in single crystal form.
The main reason is that MOFs based on these metal ions of high valence are difficult to crystallize.
Occasionally, MOFs in the form of crystalline powder were obtained, but structure solution and refinement based on Powder X-Ray Diffraction (PXRD) data is not straightforward.
Furthermore, the incorporation of rarely reported metal nodes into MOFs is less predictable and controllable.
However, metal organic (framework) powder material has been prepared by various methods but prior to the present invention large single crystals of metal organic frameworks containing a number of different metal ions have not been prepared.
In fact, serious difficulties have been experienced preparing crystalline metal organic frameworks containing aluminium.
The sizes of the crystals obtained were however relatively small.
Ferey et al therefore fail to provide aluminium MOFs having a large crystal size.
U.S. Pat. No. 8,648,002 therefore fails to prepare an aluminium MOF which is crystalline, let alone which is polycrystalline or monocrystalline and having large crystal sizes.
All these references highlight that despite a significant effort to prepare aluminium MOFs exhibiting large crystal sizes and monocrystalline characteristics, all such attempts have failed.
There are therefore clearly great difficulties associated with the preparation of aluminium metal organic framework materials having the desired properties.
Large single crystals are very rare in nature and can be difficult to produce in the laboratory.

Method used

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Examples

Experimental program
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Effect test

example 1

Synthesis of Al3O(ABTC)6-PCN 250 (Al)

[0230]

[0231]10 mg of [Al3O(OOCCH3)6.3CH3CN][AlCl4] and 10 mg of ABTC were dissolved in 2 ml of DMF, then 0.5 ml of acetic acid was added. The solution was sealed in a 4 ml vial and put into oven at 150° C. for 5 days. After cooling down to room temperature, light yellow crystals were harvested.

[0232]Optical microscope images of PCN-250 (Al) (Example 1) are shown in FIGS. 2-4. Crystal sizes of 42 μm, 10 μm, and 72 μm respectively were observed.

[0233]The crystal data and structure refinements for a single crystal of PCN-250 (Al) (Example 1) are shown in Table 1.

[0234]

TABLE 1PCN-250-AlFormulaC9 H6 Al O5.33Formula weight226.45Crystal Color / ShapeLight Yellow BlockCrystal SystemCubicSpace GroupP43na (Å)21.6035(10)V (Å3)10082.60(8)Z24dcalcd. (g / cm3)0.895μ(mm−1)0.121F(000)2776θmax [deg]26.37Completeness98.8%Collected reflections3427Unique reflections3238Parameters145Restraints3Rint0.0308R1[I > 2σ(I)]0.0386wR2 [I > 2σ(I)]0.1241R1 (all data)0.0408wR2 (all ...

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Abstract

The invention relates to monocrystalline single crystals of metal-organic framework materials comprising at least one aluminum metal ion, processes for preparing the same, methods for employing the same, and the use thereof. The invention also relates to monocrystalline aluminum metal-organic frameworks.

Description

STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT[0001]This invention was made with government support under DE-AR0000073 awarded by the U.S. Dept. of Energy. The government has certain rights in the invention.FIELD OF THE INVENTION[0002]The present invention relates to aluminium metal-organic frameworks, processes for preparing the same and the use thereof as well as aluminium metal-organic frameworks in crystalline form. In particular, the invention relates to polycrystalline and monocrystalline aluminium metal organic frameworks and to a method for preparing the same. More specifically, it relates to massive single crystal aluminium metal organic frameworks and to their methods of preparation.BACKGROUND OF THE INVENTION[0003]Metal-Organic Frameworks (MOFs) have garnered significant interests in the last two decades due to their promising potential in many applications such as gas adsorption, separation, catalysis and sensing. For example, see Yaghi, O. M.; O'Keeffe,...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): B01D53/02C07F5/06B01J20/28C01B3/50C01B3/00B01J20/22C01B31/20C01B21/04C07C7/13C01B32/50
CPCC07F15/025C07F15/045C07F15/065C07F5/069C07F7/006C01B31/20C01B21/0455C01B3/508C07C7/13B01J20/28069B01J20/28057B01J20/226C01B3/0015C01B2210/0015B01J20/28061B01J20/28066B01J20/28071B01J20/28073B01J20/28076C07F7/003C01B32/50Y02E60/32Y02C20/40C07F5/06C07F7/28C07F15/02C07F15/04C07F15/06C01B32/914
Inventor ZHOU, HONG-CAIFENG, DAWEIWANG, KECHENG
Owner TEXAS A&M UNIVERSITY
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